CN108285563A - A kind of preparation method of compliant rubber powder - Google Patents
A kind of preparation method of compliant rubber powder Download PDFInfo
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- CN108285563A CN108285563A CN201711473046.5A CN201711473046A CN108285563A CN 108285563 A CN108285563 A CN 108285563A CN 201711473046 A CN201711473046 A CN 201711473046A CN 108285563 A CN108285563 A CN 108285563A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L21/00—Compositions of unspecified rubbers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The present invention provides a kind of preparation method of compliant rubber powder, including：TMPTMA is dissolved in acetone, rubber powder is then added, it is dry after stirring, obtain modified glue powder；Modified glue powder, softening agent, activator, antioxidant, filler and plasticiser are put into agitating device, low-pressure steam is passed through, stirs, compliant rubber powder is obtained after reaction.The present invention is using two thiuram of curing and zinc stearate as activator, while deep cut-out vulcanization crosslinking network, reduces the bond energy of cross-bond, shortens the reaction time of reclaimed rubber, improve scrap rubber reclaimation efficiency.The addition of coumarone indene resin not only increases the plasticity of reclaimed rubber, plays immersional wetting, gos deep into inside rubber powder so that reaction is more abundant.Reaction in-situ can occur for the TMPTMA being added in glue powder system, and cross-linking reaction is easy to happen between TMPTMA molecules and rubber powder, enhance the vulcanized network of molded rubber, greatly improve the tensile property of rubber.
Description
Technical field
The present invention relates to material forming processing technology field more particularly to a kind of preparation methods of compliant rubber powder.
Background technology
In recent years, China about generates 1,000,000 tons of scrap rubber rubber every year, and main source is the tire scrapped, sebific duct, glue
The production of the products such as band, sole, industrial glue sundries and the material of rubber plant, some places are using waste old as fuel and coal
Burning is mixed, serious secondary pollution and the waste of resource are caused, the recycling of waste old not only expands rubber raw materials source, drop
Low production cost, and can be turned waste into wealth with environmental protection.
The recovery process of vulcanizate mostly uses greatly mechanochemical reaction at present, and disulphide is added in waste old, and such as two
Vulcanize hexichol, dibenzyl disulfide etc., these regenerative agents can not only cause damages to environment, since it contains active sulphur, when being heated
Part C-C keys can be made to be broken, obtained reclaimed rubber performance is unstable, so how to recycle to stability and high efficiency waste and old rubber
The developing direction of future rubber industry when glue.
Invention content
The main purpose of the present invention is to provide a kind of preparation method of compliant rubber powder, infiltrations good with plasticity
The feature that property is good, intensity is high.
To achieve the above objectives, the technical solution adopted by the present invention is：
A kind of preparation method of compliant rubber powder, includes the following steps：TMPTMA is dissolved in acetone, rubber is then added
Powder, it is dry after stirring, obtain modified glue powder；By modified glue powder described in 80-120 parts by weight, 8-12 parts by weight softening agent, 3-8
Parts by weight activator, 1-5 parts by weight antioxidant, 5-10 parts of filler material by weight and 5-10 parts by weight plasticisers are put into agitating device,
It is passed through low-pressure steam, stirs, compliant rubber powder, reaction pressure 0.08-0.2MPa, reaction time 30- is obtained after reaction
60min, the softening agent be paraffin oil and coumarone indene resin mixture, the activator be tetramethylthiuram disulfide with
The mixture of zinc stearate.
Preferably, the rubber powder is prepared as follows：Waste and used rubber tyre is cleaned, dry, is ground, is obtained
The thick rubber powder of tyre surface；It by the thick rubber powder first time iron removal by magnetic separation of the tyre surface, screens, crushes, second of iron removal by magnetic separation obtains rubber powder
Body.
Preferably, the weight ratio of the paraffin oil and coumarone indene resin is 3:2.
Preferably, the weight ratio of the tetramethylthiuram disulfide and zinc stearate is 1:10.
Preferably, the antioxidant is anti-aging agent RD.
Preferably, the filler is sepiolite.
Preferably, the plasticiser is o-phthalic acid dibutyl ester.
Preferably, in the step of obtaining modified glue powder, mixing time 40-70min.
Preferably, in the step of obtaining compliant rubber powder, reaction pressure 0.1MPa.
Preferably, in the step of obtaining compliant rubber powder, reaction time 45min.
The present invention provides a kind of preparation method of compliant rubber powder, includes the following steps：TMPTMA is dissolved in acetone
In, rubber powder is then added, it is dry after stirring, obtain modified glue powder；By the part by weight modified rubber powders of 80-120,8-12 parts by weight
Softening agent, 3-8 parts by weight activator, 1-5 parts by weight antioxidant, filler and plasticiser are put into agitating device, are passed through low pressure steaming
Vapour, stirring, obtains compliant rubber powder after reaction.Compared with prior art, first, the present invention is with two thiuram of curing and firmly
Resin acid zinc as activator, can deeper into cut-out vulcanization crosslinking network while, reduce the bond energy of cross-bond, shorten
The reaction time of reclaimed rubber improves scrap rubber reclaimation efficiency.Second, the addition of coumarone indene resin not only increases reclaimed rubber
Plasticity plays immersional wetting to a certain extent so that activator can more go deep into inside rubber powder so that reaction is more
Fully.Third is added to the TMPTMA molecules in glue powder system in rubber powder forming process, reaction in-situ can occur,
It is easy to happen cross-linking reaction between TMPTMA molecules and rubber powder, enhances the vulcanized network of molded rubber, greatly the drawing of rubber
Stretch performance.Therefore, the compliant rubber powder that prepared by the present invention has the characteristics that good plasticity, good penetrability, intensity are high.
Specific implementation mode
It is described below for disclosing the present invention so that those skilled in the art can realize the present invention.It is excellent in being described below
Embodiment is selected to be only used as illustrating, it may occur to persons skilled in the art that other obvious modifications.
The present invention provides a kind of preparation method of compliant rubber powder, includes the following steps：TMPTMA is dissolved in acetone, so
Rubber powder is added afterwards, it is dry after stirring, obtain modified glue powder；By modified glue powder, 8-12 parts by weight described in 80-120 parts by weight
Softening agent, 3-8 parts by weight activator, 1-5 parts by weight antioxidant, 5-10 parts of filler material by weight and 5-10 parts by weight plasticisers are put into and stir
It mixes in device, is passed through low-pressure steam, stir, compliant rubber powder, reaction pressure 0.08-0.2MPa, reaction are obtained after reaction
Time is 30-60min, and the softening agent is the mixture of paraffin oil and coumarone indene resin, and the activator is curing tetramethyl
The mixture of base thiuram and zinc stearate.
Preferably, the rubber powder is prepared as follows：Waste and used rubber tyre is cleaned, dry, is ground
Mill, obtains the thick rubber powder of tyre surface；It by the thick rubber powder first time iron removal by magnetic separation of the tyre surface, screens, crushes, second of iron removal by magnetic separation obtains
To rubber powder.
The present invention directly carries out chemical plastics processing to rubber powder, and vulcanization can be cut off in the case where not destroying rubber backbone
Cross-bond in rubber improves the intensity of reclaimed rubber so as to improve the permeability of itself and raw rubber.
Preferably, the weight ratio of the paraffin oil and coumarone indene resin is 3:2.The tetramethyl autumn is blue
The weight ratio of nurse and zinc stearate is 1:10.The antioxidant is anti-aging agent RD.The filler is sepiolite.The plasticiser is
O-phthalic acid dibutyl ester.
Activator of the present invention use curing two thiurams and zinc stearate combination, can deeper into cut-out vulcanize hand over
While networking network, the bond energy of cross-bond is reduced, the reaction time of reclaimed rubber is shortened, improves scrap rubber reclaimation efficiency.It is ancient
The addition of the grand resin of horse not only increases the plasticity of reclaimed rubber, plays immersional wetting to a certain extent so that activation
Agent can more be goed deep into inside rubber powder so that reaction is more abundant.Due to the addition of sepiolite, reclaimed rubber is considerably increased mixed
Frictional force when conjunction so that rubber powder is more abundant in mixing, reduces energy consumption while improving efficiency.In addition the addition of DOP
The interaction of activator and rubber is strengthened, while also improving the plasticity of rubber.
Preferably, in the step of obtaining modified glue powder, mixing time 40-70min.Obtain compliant rubber powder
The step of in, reaction pressure 0.1MPa；Reaction time is 45min.The present invention is added to the TMPTMA molecules in glue powder system
In rubber powder forming process, reaction in-situ can occur, be easy to happen cross-linking reaction between TMPTMA molecules and rubber powder, enhance
The vulcanized network of molded rubber, the greatly tensile property of rubber.
From above scheme as can be seen that the present invention recycles waste old using a kind of completely new regeneration technology, obtain
Green, plasticity and the high recycling rubber powder of good penetrability, intensity are arrived.
For a further understanding of the present invention, technical solution provided by the invention is carried out specifically with reference to embodiment
Bright, protection scope of the present invention is not limited by the following examples.
Raw material and chemical reagent used in the embodiment of the present invention are purchased in market.
The softening agent is the mixture of common commercially available paraffin oil and coumarone indene resin, ratio 3:2；
The activator is the mixture of tetramethylthiuram disulfide and zinc stearate, ratio 1:10；
The antioxidant is common commercially available anti-aging agent RD；
The filler is sepiolite；
The plasticiser is o-phthalic acid dibutyl ester (DOP), producer：Shandong Ke Xing Chemical Co., Ltd.s；
The modifying agent is trimethylol-propane trimethacrylate (TMPTMA), producer：Sigma-Aldrich,
CAS：3290-92-4.
Embodiment 1
Waste and used rubber tyre is subjected to cleaning 10-20min, it is to be cleaned it is clean after dry；
By the waste and used rubber tyre dried in board top bevel, and collect the thick rubber powder of tyre surface；
Tyre surface coarse powder carries out the tyre surface coarse powder after iron removal by magnetic separation is screened；
Tyre surface coarse powder after screening pulverizer is crushed into (40-60 mesh), is packaged rubber powder after carrying out secondary iron removal by magnetic separation.
5 parts by weight TMPTMA are dissolved in acetone, the rubber powder after secondary iron removal by magnetic separation is put into stirring at normal temperature 40-
It is dry after 70min, it does spare in next step.
100 parts by weight of rubber powder, 10 parts by weight of softening agent, 5 parts by weight of regeneration activator, 2 parts by weight of antioxidant, filler 10
Parts by weight and 10 parts by weight of plasticiser are put into mixing plant, are passed through low-pressure steam, are sufficiently stirred 45min, and container pressure maintains
In 0.1MPa, reaction time 45min, after packing packaging carried out by air intake device sucking charging hopper, obtain compliant rubber
Powder.
Detect its tensile strength be 16MPa, ash content 10%, the elongation at break variation of Mooney on the 500%, 15 (△ ML)
It is 1.
Embodiment 2
Waste and used rubber tyre is subjected to cleaning 10-20min, it is to be cleaned it is clean after dry；
By the waste and used rubber tyre dried in board top bevel, and collect the thick rubber powder of tyre surface；
Tyre surface coarse powder carries out the tyre surface coarse powder after iron removal by magnetic separation is screened；
Tyre surface coarse powder after screening pulverizer is crushed into (40-60 mesh), is packaged rubber powder after carrying out secondary iron removal by magnetic separation.
3 parts by weight TMPTMA are dissolved in acetone, the rubber powder after secondary iron removal by magnetic separation is put into stirring at normal temperature 40-
It is dry after 70min, it does spare in next step.
100 parts by weight of rubber powder, 5 parts by weight of softening agent, 2 parts by weight of regeneration activator, 1 parts by weight of antioxidant, 5 weight of filler
Amount part and 10 parts by weight of plasticiser are put into mixing plant, are passed through low-pressure steam, are sufficiently stirred 45min, container pressure maintains
0.1MPa, reaction time 45min, after by air intake device sucking charging hopper carry out packing packaging, obtain compliant rubber powder.
Detect its tensile strength be 14MPa, ash content 10%, the elongation at break variation of Mooney on the 450%, 15 (△ ML)
It is 4.
Embodiment 3
Waste and used rubber tyre is subjected to cleaning 10-20min, it is to be cleaned it is clean after dry；
By the waste and used rubber tyre dried in board top bevel, and collect the thick rubber powder of tyre surface；
Tyre surface coarse powder carries out the tyre surface coarse powder after iron removal by magnetic separation is screened；
Tyre surface coarse powder after screening pulverizer is crushed into (40-60 mesh), is packaged rubber powder after carrying out secondary iron removal by magnetic separation；
1 parts by weight TMPTMA is dissolved in acetone, the rubber powder after secondary iron removal by magnetic separation is put into stirring at normal temperature 40-
It is dry after 70min, it does spare in next step.
100 parts by weight of rubber powder, 20 parts by weight of softening agent, 10 parts by weight of regeneration activator, 4 parts by weight of antioxidant, filler 5
Parts by weight and 10 parts by weight of plasticiser are put into mixing plant, are passed through low-pressure steam, are sufficiently stirred 45min, and container pressure maintains
In 0.1MPa, reaction time 45min, after packing packaging carried out by air intake device sucking charging hopper, obtain compliant rubber
Powder.
Detect its tensile strength be 11MPa, ash content 10%, the elongation at break variation of Mooney on the 500%, 15 (△ ML)
It is 6.
Comparative example
Using the preparation method of embodiment 1, the raw material and performance of use are as shown in table 1.
The raw material and the performance test results that 1 comparative example of the present invention of table uses
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection domain by appended claims and its
Equivalent defines.
Claims (10)
1. a kind of preparation method of compliant rubber powder, which is characterized in that include the following steps：
TMPTMA is dissolved in acetone, rubber powder is then added, it is dry after stirring, obtain modified glue powder；
By modified glue powder described in 80-120 parts by weight, 8-12 parts by weight softening agent, 3-8 parts by weight activator, 1-5 parts by weight antioxygens
Agent, 5-10 parts of filler material by weight and 5-10 parts by weight plasticisers are put into agitating device, are passed through low-pressure steam, stirring, after reaction
To compliant rubber powder, reaction pressure 0.08-0.2MPa, reaction time 30-60min,
The softening agent is the mixture of paraffin oil and coumarone indene resin,
The activator is the mixture of tetramethylthiuram disulfide and zinc stearate.
2. preparation method according to claim 1, which is characterized in that the rubber powder is prepared as follows：
Waste and used rubber tyre is cleaned, dry, is ground, the thick rubber powder of tyre surface is obtained；
It by the thick rubber powder first time iron removal by magnetic separation of the tyre surface, screens, crushes, second of iron removal by magnetic separation obtains rubber powder.
3. preparation method according to claim 1, which is characterized in that the weight ratio of the paraffin oil and coumarone indene resin is
3:2。
4. preparation method according to claim 1, which is characterized in that the tetramethylthiuram disulfide and zinc stearate
Weight ratio be 1:10.
5. preparation method according to claim 1, which is characterized in that the antioxidant is anti-aging agent RD.
6. preparation method according to claim 1, which is characterized in that the filler is sepiolite.
7. preparation method according to claim 1, which is characterized in that the plasticiser is o-phthalic acid dibutyl ester.
8. preparation method according to claim 1, which is characterized in that in the step of obtaining modified glue powder, mixing time is
40-70min。
9. preparation method according to claim 1, which is characterized in that in the step of obtaining compliant rubber powder, reaction pressure
Power is 0.1MPa.
10. preparation method according to claim 1, which is characterized in that in the step of obtaining compliant rubber powder, when reaction
Between be 45min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711473046.5A CN108285563A (en) | 2017-12-29 | 2017-12-29 | A kind of preparation method of compliant rubber powder |
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| CN201711473046.5A CN108285563A (en) | 2017-12-29 | 2017-12-29 | A kind of preparation method of compliant rubber powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4166608A1 (en) * | 2021-10-12 | 2023-04-19 | A.G.R. S.r.l. | Rubber composition with low odor emissions and process for its production |
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| EP1234846A1 (en) * | 2000-06-15 | 2002-08-28 | China Petroleum & Chemical Corporation | Silicone rubber in the form of a finely divided powder, method for the production and the use of the same |
| CN101948579A (en) * | 2010-10-25 | 2011-01-19 | 曾广胜 | Method for preparing all-rubber powder elastic body from waste rubber |
| CN103849070A (en) * | 2014-03-06 | 2014-06-11 | 汉川市童宝童车有限公司 | Olefin thermoplastic elastomer and preparation method thereof |
| CN105968581A (en) * | 2016-07-01 | 2016-09-28 | 湖北洋田塑料制品有限公司 | Thermoplastic elastomer for children's vehicles and preparation method of thermoplastic elastomer |
| CN106810742A (en) * | 2016-12-22 | 2017-06-09 | 北京绿源国瑞科技股份有限公司 | A kind of modified glue powder/regenerated polythene insulating tube composite and preparation method thereof |
-
2017
- 2017-12-29 CN CN201711473046.5A patent/CN108285563A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1234846A1 (en) * | 2000-06-15 | 2002-08-28 | China Petroleum & Chemical Corporation | Silicone rubber in the form of a finely divided powder, method for the production and the use of the same |
| CN101948579A (en) * | 2010-10-25 | 2011-01-19 | 曾广胜 | Method for preparing all-rubber powder elastic body from waste rubber |
| CN103849070A (en) * | 2014-03-06 | 2014-06-11 | 汉川市童宝童车有限公司 | Olefin thermoplastic elastomer and preparation method thereof |
| CN105968581A (en) * | 2016-07-01 | 2016-09-28 | 湖北洋田塑料制品有限公司 | Thermoplastic elastomer for children's vehicles and preparation method of thermoplastic elastomer |
| CN106810742A (en) * | 2016-12-22 | 2017-06-09 | 北京绿源国瑞科技股份有限公司 | A kind of modified glue powder/regenerated polythene insulating tube composite and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4166608A1 (en) * | 2021-10-12 | 2023-04-19 | A.G.R. S.r.l. | Rubber composition with low odor emissions and process for its production |
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Application publication date: 20180717 |